CN101177742A - Method for in-situ preparation of TiBO2 reinforced magnesium-based composite material - Google Patents
Method for in-situ preparation of TiBO2 reinforced magnesium-based composite material Download PDFInfo
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- CN101177742A CN101177742A CNA200710047943XA CN200710047943A CN101177742A CN 101177742 A CN101177742 A CN 101177742A CN A200710047943X A CNA200710047943X A CN A200710047943XA CN 200710047943 A CN200710047943 A CN 200710047943A CN 101177742 A CN101177742 A CN 101177742A
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Abstract
The invention relates to a method of in-situ preparing TiB2 granule strengthening Mg-based composite material in the composite material technical field. The steps are that: powder of K2TiF6, KBF4 and Na3AlF6 are mixed uniformly and then put into a kiln for drying, thus obtaining waterless powder. Aluminum ingot is melted in a resistance furnace with heat preservation and uniformity; the waterless powder after dried is added to the melting Al melt liquid by batch and then is stirred with a graphite disc, and scum on the surface of the melt liquid is removed after stirred and stewed, thus obtaining TiB2-Al intermediate alloy; magnesium alloy is smelted with the protection of SF6 and CO2 mixing gas, and flame retardant element beryllium is added; the TiB2-Al intermediate alloy is added into the magnesium alloy melting solution slowly, stirred, stewed and cast. The technology of the invention is comparatively simple, has low cost, and the density of TiB2/Mg composite material is between 1.8-2.0g/cm<3> and tensile strength thereof is increased by more than 60 percent than base alloy.
Description
Technical field
That the present invention relates to is a kind of preparation method of technical field of composite materials, particularly a kind of in-situ preparing TiB
2The method of particle reinforced magnesium base compound material.
Background technology
Magnesium base composite material is owing to have high specific tenacity, specific modulus and good abrasion resistance, and resistance to elevated temperatures and damping capacity, in aerospace, automotive industry has potential application prospect and vast market.The previous research work of magnesium base composite material mainly concentrates on the magnesium base composite material that adds the method preparation, but because wettability is relatively poor between enhancing body and the matrix alloy, unstable on wild phase and the basal body interface thermodynamics, add the difference of specific gravity of the two simultaneously and cause the poly-partially easily and gathering of particle in the Composite Preparation process, the preparation difficulty that further causes magnesium base composite material, complex process, performance of composites can't be compared with the performance of expection.Problems such as employing in-situ preparing particle reinforced magnesium base compound material can solve the surface reaction that outer addition produces, and wettability difference and strengthening effect are limited.Therefore the research of original position magnesium base composite material is in recent years extremely paid attention to.Many investigators have begun the exploration of this respect.But with respect to the development that adds magnesium base composite material and in-situ Al-base, titanium matrix composite, the research and development of in-situ authigenic magnesium base composite material just begins, and relevant research, report also will be done a large amount of work not enough.The matter of utmost importance of the urgent solution that the original position magnesium base composite material is faced is exactly the further perfect of preparation technology.Consider the easy reactivity of magnesium, easy firing, perishable, magnesium matrix and the infiltrating restriction that strengthens body, the essential characteristic of magnesium base composite material has limited the selection of process means.The in-situ preparing technical development till now, existing ten several different methods, but can in magnesium base composite material, use very limited.
Through the literature search of prior art being found around method of preparing magnesium-based composite material, many bibliographical informations are arranged, as Chinese patent application number 03116169.3, name is called: " mixed salt method prepares original position and strengthens magnesium base composite material technology ".The technical characterstic of this patent stirs cast after being mixing salt directly added the magnesium melt, obtains the original position magnesium base composite material.But magnesium is burning easily at high temperature, and mixing salt directly adds in the magnesium melt, and to reaction atmosphere, temperature of reaction has strict requirement, and is wayward in actual production, has certain limitation so above-mentioned original position strengthens magnesium base composite material technology.
Summary of the invention
The present invention seeks at the deficiencies in the prior art, a kind of in-situ preparing TiB is provided
2The method of particle reinforced magnesium base compound material makes it adopt the conventional cast legal system to be equipped with original position and generates particle reinforced magnesium base compound material, has saved wild phase and has synthesized separately, handles and the adding supervisor, thereby had advantages such as technology is simple, preparation cost is low.
The present invention is achieved by the following technical solutions, adopts casting to prepare TiB
2Particle reinforced magnesium base compound material is by the generated in-situ TiB of mixing salt reaction method
2-Al master alloy adds in the molten magnesium liquid and use stirring cast forms.Simple for process, the wild phase of generation is stable, does not contain intermediate phase, and technological process comprises that the preparation of master alloy and dissolving diffusion and the disperse of enhanced granule in magnesium alloy substrate distribute.
The present invention includes following steps:
(1) with K
2TiF
6, KBF
4And Na
3AlF
6Powder mixes is even, puts into stoving oven and dries, and obtains anhydrous powder;
(2) in resistance furnace, the Al ingot is melted, and the insulation homogenizing;
(3) step (1) is obtained on the fusion Al melt liquid level middle in batches the adding in the step (2) through the anhydrous powder of drying, and stir, leave standstill after the stirring end, remove the scum silica frost of bath surface, the TiB that obtains with graphite disk
2-Al master alloy;
(4) magnesium alloy is at SF
6And CO
2Melting under the protection of mixed gas, and add the ignition-proof element beryllium to prevent the magnesium burning;
(5) with the TiB that obtains in the step (3)
2-Al master alloy slowly joins in the magnesium alloy liquation that obtains in the step (4), stirs, and leaves standstill cast.
In the step (1), described K
2TiF
6And KBF
4Press Ti: the B stoichiometric mixes Na at 1: 2
3AlF
6Content is for adding K
2TiF
6, KBF
4And Na
3AlF
6The 5%-20% of powder gross weight, the bake out temperature of powder and time are: 100 ℃-250 ℃, 1 hour-5 hours.
In the step (2), described Al ingot heat fused temperature is 700 ℃-850 ℃, and the insulation homogenization time is 10 minutes-30 minutes.
In the step (3), describedly stir with graphite disk, its stirring velocity scope is at 200r/min-1000r/min, and churning time is 10 minutes-60 minutes, wait to stir stop after, time of repose is 10 minutes-30 minutes.
In the step (4), described magnesium alloy smelting temperature is 700 ℃-850 ℃.
In the step (5), described mixing speed is 200r/min-1000r/min, and churning time is 10 minutes-60 minutes, and time of repose is 5 minutes-30 minutes.
The present invention generates TiB by the mixed salt method original position earlier in aluminium
2-Al master alloy is again with fused TiB
2-Al master alloy adds in the magnesium of molten state, obtains TiB
2/ Mg matrix material.TiB
2Particle is at TiB
2Be purified in the-Al master alloy and surface coverage has aluminium, institute is so that TiB
2Particle can have good wettability in magnesium alloy.TiB
2Particle can pass through TiB easily
2-Al master alloy fuses into magnesium alloy and is evenly distributed in the matrix.
Compare with present existing technology, the present invention adopts casting to prepare original position and generates particle enhancing TiB
2/ Mg matrix material has overcome and has added the easily oxidation stain of enhanced granule surface, with the wettability difference of matrix and particle is thick and skewness, easily gathers in problems such as crystal boundaries partially, thereby has advantages such as technology is simple, preparation cost is low.Because TiB
2Enhanced granule is reflected at reaction generation in the metallic aluminium through mixing salt, and is good with the matrix wettability, fully stirs the back and is evenly distributed in matrix, the wild phase particle is tiny, and reinforced effects is remarkable, and the interface is in conjunction with good, technology is simple, is easy to control, so original position generates particle enhancing TiB
2/ Mg matrix material has the characteristics of high-strength light.TiB
2/ Mg composite density is at 1.8-2.0g/cm
3Between, its tensile strength has increased more than 60% than matrix alloy.The present invention realizes that for the in-situ preparing of magnesium base composite material many body system, multiplex's skill provide effective ways.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Produce 4vol%TiB
2Strengthen magnesium base composite material
With powder K
2TiF
6And KBF
4And sodium aluminum fluoride Na
3AlF
6Mix.Two kinds of salt K
2TiF
6And KBF
4Stoichiometric ratio according to Ti: B is mixed sodium aluminum fluoride Na at 1: 2
3AlF
6Content is the 5wt% of powder total amount, mixes the back 250 ℃ of preheatings 1 hour.The metal aluminium ingot is heated to fusing about 850 ℃, and is incubated homogenizing 10 minutes.Mixed powder is added in the fused aluminium and stirs with the speed of 200r/min, and churning time is 60 minutes.After stirring stops, leaving standstill 20 minutes, slagging-off obtains TiB
2-Al master alloy.Magnesium alloy is at mixed gas SF
6And CO
2Protection under 800 ℃ of meltings.After magnesium alloy melts, TiB
2In the magnesium alloy that-Al master alloy is slowly added.Implement to stir, mixing speed is 200r/min, churning time 30 minutes.After the stirring, left standstill casting 5 minutes.Obtain 4vol%TiB
2/ Mg matrix material, its tensile strength are 300MPa.
Embodiment 2,
Produce 2vol%TiB
2Strengthen magnesium base composite material
With K
2TiF
6And KBF
4And sodium aluminum fluoride Na
3AlF
6Powder mixes is even.Two kinds of salt K
2TiF
6And KBF
4Stoichiometric ratio according to Ti: B is mixed sodium aluminum fluoride Na at 1: 2
3AlF
6Content is the 20wt% of powder total amount, mixes the back 100 ℃ of preheatings 5 hours.The Al ingot is heated to fusing about 800 ℃, and is incubated homogenizing 30 minutes.Mixed powder is added in the fused aluminium and constantly and stirs.Churning time is 10min, and stirring velocity is 1000rpm.After stirring stops, leaving standstill 10 minutes, slagging-off obtains TiB
2-Al master alloy.Magnesium alloy is at mixed gas SF
6And CO
2Protection under 700 ℃ of meltings.After magnesium alloy melts, TiB
2-Al master alloy is slowly added in the magnesium alloy that constantly stirs.Stirred 10 minutes, stirring velocity is 1000rpm.After stirring stops, leaving standstill 60 minutes cast.Obtain 2vol%TiB
2/ Mg matrix material, its tensile strength 290MPa.
Embodiment 3
Produce 1vol%TiB
2Strengthen magnesium base composite material
With K
2TiF
6And KBF
4And sodium aluminum fluoride Na
3AlF
6Powder mixes is even.Two kinds of salt K
2TiF
6And KBF
4Stoichiometric ratio according to Ti: B is mixed sodium aluminum fluoride Na at 1: 2
3AlF
6Content is the 10wt% of mixed powder total amount, mixes the back 200 ℃ of preheatings 3 hours.The Al ingot is heated to fusing about 700 ℃, and is incubated homogenizing 20 minutes.Mixed powder is added in the fused aluminium and implements and stirs.Churning time is 30min, and stirring velocity is 400rpm.Stop after the reaction stirring, left standstill 30 minutes, slagging-off obtains TiB
2-Al master alloy.Magnesium alloy is at mixed gas SF
6And CO
2Protection under 850 ℃ of meltings.After magnesium alloy melts, TiB
2-Al master alloy is slowly added in the fused magnesium alloy.Stirred 60 minutes, stirring velocity is 600rpm.After stirring end, left standstill 10 minutes cast.Obtain 1vol%TiB
2/ Mg matrix material, its tensile strength 270MPa.
Claims (10)
1. in-situ preparing TiB
2The method of particle reinforced magnesium base compound material is characterized in that, may further comprise the steps:
(1) with K
2TiF
6, KBF
4And Na
3AlF
6Powder mixes is even, puts into stoving oven and dries, and obtains anhydrous powder, wherein: K
2TiF
6And KBF
4Press Ti: the B stoichiometric mixes Na at 1: 2
3AlF
6Content is for adding K
2Ti
F6, KBF
4And Na
3AlF
6The 5%-20% of powder gross weight;
(2) in resistance furnace, the Al ingot is melted, and the insulation homogenizing;
(3) step (1) is obtained on the fusion Al melt liquid level middle in batches the adding in the step (2) through the anhydrous powder of drying, and stir, leave standstill after the stirring end, remove the scum silica frost of bath surface, the TiB that obtains with graphite disk
2-Al master alloy;
(4) magnesium alloy is at SF
6And CO
2Melting under the protection of mixed gas, and add the ignition-proof element beryllium to prevent the magnesium burning;
(5) with the TiB that obtains in the step (3)
2-Al master alloy slowly joins in the magnesium alloy liquation that obtains in the step (4), stirs, and leaves standstill cast.
2. in-situ preparing TiB according to claim 1
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (1), and described oven dry, its temperature is 100 ℃-250 ℃, the time is 1 hour-5 hours.
3. in-situ preparing TiB according to claim 1
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (2), described Al ingot heat fused temperature is 700 ℃-850 ℃.
4. according to claim 1 or 3 described in-situ preparing TiB
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (2), and described insulation homogenizing, its time is 10 minutes-30 minutes.
5. in-situ preparing TiB according to claim 1
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (3), described with the graphite disk stirring, its stirring velocity scope is at 200r/min-1000r/min.
6. in-situ preparing TiB according to claim 1 or 5
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (3), and described stirring, its time is 10 minutes-60 minutes,
7. in-situ preparing TiB according to claim 1 or 5
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (3), and described leaving standstill, its time is 10 minutes-30 minutes.
8. in-situ preparing TiB according to claim 1
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (4), described magnesium alloy smelting temperature is 700 ℃-850 ℃.
9. in-situ preparing TiB according to claim 1
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (5), and described stirring, its rotating speed is 200r/min-1000r/min, churning time is 10 minutes-60 minutes.
10. according to claim 1 or 9 described in-situ preparing TiB
2The method of particle reinforced magnesium base compound material is characterized in that: in the step (5), and described leaving standstill, its time is 5 minutes-30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710047943XA CN101177742A (en) | 2007-11-08 | 2007-11-08 | Method for in-situ preparation of TiBO2 reinforced magnesium-based composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710047943XA CN101177742A (en) | 2007-11-08 | 2007-11-08 | Method for in-situ preparation of TiBO2 reinforced magnesium-based composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101177742A true CN101177742A (en) | 2008-05-14 |
Family
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352449A (en) * | 2011-10-12 | 2012-02-15 | 南昌大学 | Preparation method of in-situ ZrB2 particle reinforced magnesium-based composite |
| WO2013023460A1 (en) * | 2012-03-07 | 2013-02-21 | 深圳市新星轻合金材料股份有限公司 | Cycled preparation method that uses mixture of sodium-based titanium and boron fluoride salts as intermediate raw material and produces titanium boride and simultaneously sodium cryolite |
| CN103031475A (en) * | 2012-12-28 | 2013-04-10 | 山东大学 | In-situ synthesized Al3BC reinforced magnesium matrix composite and fabrication method thereof |
| CN103160777A (en) * | 2011-12-15 | 2013-06-19 | 中国科学院宁波材料技术与工程研究所 | Titanium diboride-nickel thin film with coating structure and preparation method thereof |
| CN105568074A (en) * | 2016-03-09 | 2016-05-11 | 哈尔滨工业大学（威海） | Preparation method of in-situ aluminum matrix composite |
| CN109943738A (en) * | 2019-05-15 | 2019-06-28 | 湖南科技大学 | One kind magnesium-rare earth of high-modulus containing aluminium and preparation method thereof |
| CN110938759A (en) * | 2019-11-26 | 2020-03-31 | 纽维科精密制造江苏有限公司 | Production process of in-situ self-generated aluminum-based composite material for aluminum profile |
| CN111822722A (en) * | 2020-06-30 | 2020-10-27 | 长沙新材料产业研究院有限公司 | TiAl/TiB for additive manufacturing2Method for preparing powder material |
| CN113798494A (en) * | 2021-08-12 | 2021-12-17 | 山东科技大学 | TiB2Particle reinforced magnesium-based composite material and preparation method thereof |
-
2007
- 2007-11-08 CN CNA200710047943XA patent/CN101177742A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352449A (en) * | 2011-10-12 | 2012-02-15 | 南昌大学 | Preparation method of in-situ ZrB2 particle reinforced magnesium-based composite |
| CN103160777A (en) * | 2011-12-15 | 2013-06-19 | 中国科学院宁波材料技术与工程研究所 | Titanium diboride-nickel thin film with coating structure and preparation method thereof |
| CN103160777B (en) * | 2011-12-15 | 2014-12-17 | 中国科学院宁波材料技术与工程研究所 | Titanium diboride-nickel thin film with coating structure and preparation method thereof |
| GB2510008B (en) * | 2012-03-07 | 2015-09-09 | Shenzhen Sunxing Light Alloys Materials Co Ltd | Cyclic preparation method for producing titanium boride from intermediate feedstock Na-based Ti-B-F salt mixture and producing sodium cryolite as byproduct |
| GB2510008A (en) * | 2012-03-07 | 2014-07-23 | Shenzhen Sunxing Light Alloys Materials Co Ltd | Cycled preparation method that uses mixture of sodium-based titanium and boron fluoride salts as intermediate raw material and produces titanium boride |
| WO2013023460A1 (en) * | 2012-03-07 | 2013-02-21 | 深圳市新星轻合金材料股份有限公司 | Cycled preparation method that uses mixture of sodium-based titanium and boron fluoride salts as intermediate raw material and produces titanium boride and simultaneously sodium cryolite |
| CN103031475A (en) * | 2012-12-28 | 2013-04-10 | 山东大学 | In-situ synthesized Al3BC reinforced magnesium matrix composite and fabrication method thereof |
| CN105568074A (en) * | 2016-03-09 | 2016-05-11 | 哈尔滨工业大学（威海） | Preparation method of in-situ aluminum matrix composite |
| CN109943738A (en) * | 2019-05-15 | 2019-06-28 | 湖南科技大学 | One kind magnesium-rare earth of high-modulus containing aluminium and preparation method thereof |
| CN110938759A (en) * | 2019-11-26 | 2020-03-31 | 纽维科精密制造江苏有限公司 | Production process of in-situ self-generated aluminum-based composite material for aluminum profile |
| CN111822722A (en) * | 2020-06-30 | 2020-10-27 | 长沙新材料产业研究院有限公司 | TiAl/TiB for additive manufacturing2Method for preparing powder material |
| CN111822722B (en) * | 2020-06-30 | 2023-09-19 | 航天科工(长沙)新材料研究院有限公司 | TiAl/TiB for additive manufacturing 2 Preparation method of powder material |
| CN113798494A (en) * | 2021-08-12 | 2021-12-17 | 山东科技大学 | TiB2Particle reinforced magnesium-based composite material and preparation method thereof |
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